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Chlorosuccinimide → 1-(3-chlorotetrahydro-2H-1,3-thiazin-2-ylidene)-3-(2,4-dichlorophenoxy)-1-nitro-2-propanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | MAGNESIUM SILICATE (synthetic) | HCID 61680 | — |
| 反応物 | 3-(2,4-dichlorophenoxy)-1-nitro-1-(tetrahydro-2H-1,3-thiazin-2-ylidene)-2-propanone | HCID 86734697 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(3-chlorotetrahydro-2H-1,3-thiazin-2-ylidene)-3-(2,4-dichlorophenoxy)-1-nitro-2-propanone | HCID 53685320 | — |
反応手順
3.6 g of 1 and 2.1 g of N-chlorosuccinimide were combined in 150 ml of carbon tetrachloride and the mixture was refluxed for 1 hour. The resulting mixture was filtered through Celite and the solvent was evaporated to give a liquid, which was triturated in ether, decolorized with activated charcoal and filtered through Celite and stripped of solvent to give a yellow cloudy liquid. This was passed through Florisil, using methylene chloride as eluent; then stripped to give an oil, which was kept in a refrigerator over a week-end. Part of the oil crystallized. On scratching, more crystals formed. Separation of the crystals gave 2, as bright yellow crystals, m.p. 103°-105°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04024138 |
| 出典データセット | uspto-grants-1977_05 |
| ORD ID | ord-ef2eb43ad0c849a29ce457c530052334 |
| 出典メモ | uspto-grants-1977_05 |